supplementary materials
catena-Poly[[[diaquaterbium(III)]-
-6-carboxynicotinato-
-pyridine-2,5-dicarboxylato] dihydrate]
The title compound, {[Tb(C7H3NO4)(C7H4NO4)(H2O)2]·2H2O}n, is isotypic with the analogous TmIII compound [Li, Zhang, Wang & Bai (2009). Acta Cryst. E65, m411]. The TbIII atom is octacoordinated by two water molecules and by four carboxylate O atoms and two pyridyl N atoms from two pyridine-2,5-dicarboxylate (2,5-pydc) and two 6-carboxynicotinate (2,5-Hpydc) ligands. The 2,5-pydc and 2,5-Hpydc ligands bridge TbIII atoms, generating helical coordination polymers along [001]. An extensive network of O-H
O hydrogen bonds is formed between the coordination polymers and the uncoordinated water molecules. The refined Flack parameter of 0.54 (2) suggests inversion twinning.
A mixture of terbium oxide (0.5 mmol), pyridine-2,5-dicarboxylic acid (0.5 mmol), in H2O (8 ml) and ethanol (8 ml) was sealed in a 25 ml Teflon-lined
stainless steel autoclave and kept at 413 K for three days. Colourless
crystals were obtained after cooling to room temperature with a yield of 27%.
Elemental analysis calculated for C14H15N2TbO12: C 30.68, H 2.74, N
5.11%; Found: C 30.62, H 2.72, N 5.06%.
H atoms bound to C atoms were placed in calculated positions with C—H = 0.93 Å and refined as riding with Uiso(H) = 1.2Ueq(C). H atoms
of the water molecules were placed so as to form a reasonable H-bond network
and refined as riding with Uiso(H) = 1.5Ueq(O). The Flack
parameter was refined as a full least-squares variable, and the refined value
of 0.54 (2) suggests inversion twinning.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
catena-Poly[[[diaquaterbium(III)]-µ-6-carboxynicotinato-µ-
pyridine-2,5-dicarboxylato] dihydrate]
top
Crystal data top
| [Tb(C7H3NO4)(C7H4NO4)(H2O)2]·2H2O | Dx = 2.202 Mg m−3 |
| Mr = 562.20 | Mo Kα radiation, λ = 0.71073 Å |
| Tetragonal, I4 | Cell parameters from 3001 reflections |
| Hall symbol: I -4 | θ = 1.9–25.3° |
| a = 15.107 (2) Å | µ = 4.25 mm−1 |
| c = 14.8587 (15) Å | T = 298 K |
| V = 3391.1 (7) Å3 | Block, colourless |
| Z = 8 | 0.12 × 0.11 × 0.08 mm |
| F(000) = 2192 | |
Data collection top
Bruker APEXII CCD diffractometer | 3001 independent reflections |
| Radiation source: fine-focus sealed tube | 2886 reflections with I > 2σ(I) |
| graphite | Rint = 0.072 |
| φ and ω scans | θmax = 25.3°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −12→18 |
| Tmin = 0.617, Tmax = 0.713 | k = −18→17 |
| 6901 measured reflections | l = −13→17 |
Refinement top
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.053 | H-atom parameters constrained |
| wR(F2) = 0.131 | w = 1/[σ2(Fo2) + (0.1007P)2 + 0.8682P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.03 | (Δ/σ)max < 0.001 |
| 3001 reflections | Δρmax = 3.51 e Å−3 |
| 263 parameters | Δρmin = −1.17 e Å−3 |
| 0 restraints | Absolute structure: Flack (1983), 1387 Freidel pairs |
| Primary atom site location: structure-invariant direct methods | Flack parameter: 0.54 (2) |
Crystal data top
| [Tb(C7H3NO4)(C7H4NO4)(H2O)2]·2H2O | Z = 8 |
| Mr = 562.20 | Mo Kα radiation |
| Tetragonal, I4 | µ = 4.25 mm−1 |
| a = 15.107 (2) Å | T = 298 K |
| c = 14.8587 (15) Å | 0.12 × 0.11 × 0.08 mm |
| V = 3391.1 (7) Å3 | |
Data collection top
Bruker APEXII CCD diffractometer | 3001 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2886 reflections with I > 2σ(I) |
| Tmin = 0.617, Tmax = 0.713 | Rint = 0.072 |
| 6901 measured reflections | θmax = 25.3° |
Refinement top
| R[F2 > 2σ(F2)] = 0.053 | H-atom parameters constrained |
| wR(F2) = 0.131 | Δρmax = 3.51 e Å−3 |
| S = 1.03 | Δρmin = −1.17 e Å−3 |
| 3001 reflections | Absolute structure: Flack (1983), 1387 Freidel pairs |
| 263 parameters | Flack parameter: 0.54 (2) |
| 0 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F2, conventional R-factors R are based
on F, with F set to zero for negative F2. The threshold expression of
F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F2 are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top| | x | y | z | Uiso*/Ueq | |
| Tb1 | 0.30210 (3) | 0.22535 (3) | 0.22736 (3) | 0.01388 (17) | |
| C1 | 0.1833 (6) | 0.4100 (6) | 0.1946 (6) | 0.0116 (19) | |
| C2 | 0.1334 (7) | 0.4753 (6) | 0.1553 (6) | 0.0148 (19) | |
| H2A | 0.1128 | 0.5222 | 0.1900 | 0.018* | |
| C3 | 0.1132 (7) | 0.4720 (7) | 0.0639 (7) | 0.019 (2) | |
| H3A | 0.0796 | 0.5166 | 0.0376 | 0.023* | |
| C4 | 0.1433 (6) | 0.4021 (6) | 0.0129 (7) | 0.015 (2) | |
| C5 | 0.1879 (7) | 0.3364 (7) | 0.0575 (8) | 0.021 (2) | |
| H5A | 0.2046 | 0.2864 | 0.0251 | 0.025* | |
| C6 | 0.2161 (6) | 0.4123 (6) | 0.2921 (6) | 0.015 (2) | |
| C7 | 0.1302 (7) | 0.3959 (7) | −0.0870 (7) | 0.017 (2) | |
| C8 | 0.1196 (7) | 0.1238 (6) | 0.1716 (7) | 0.014 (2) | |
| C9 | 0.0975 (6) | 0.1488 (6) | 0.2710 (7) | 0.0129 (18) | |
| C10 | 0.0233 (6) | 0.1192 (7) | 0.3157 (7) | 0.017 (2) | |
| H10A | −0.0195 | 0.0865 | 0.2854 | 0.021* | |
| C11 | 0.0131 (7) | 0.1383 (7) | 0.4052 (7) | 0.018 (2) | |
| H11A | −0.0351 | 0.1158 | 0.4366 | 0.022* | |
| C12 | 0.0768 (6) | 0.1929 (6) | 0.4506 (6) | 0.0115 (18) | |
| C13 | 0.1449 (7) | 0.2207 (7) | 0.3980 (7) | 0.019 (2) | |
| H13A | 0.1865 | 0.2577 | 0.4249 | 0.023* | |
| C14 | 0.0684 (7) | 0.2114 (7) | 0.5505 (7) | 0.018 (2) | |
| N1 | 0.1583 (5) | 0.2001 (5) | 0.3112 (6) | 0.0142 (16) | |
| N2 | 0.2094 (5) | 0.3400 (5) | 0.1465 (6) | 0.0142 (17) | |
| O1 | 0.2739 (5) | 0.3551 (4) | 0.3099 (5) | 0.0178 (15) | |
| H1 | 0.3058 | 0.3643 | 0.3561 | 0.027* | |
| O2 | 0.1862 (6) | 0.4677 (6) | 0.3436 (5) | 0.035 (2) | |
| O3 | 0.1625 (5) | 0.3283 (5) | −0.1271 (5) | 0.0212 (16) | |
| O4 | 0.0921 (6) | 0.4561 (5) | −0.1264 (5) | 0.0262 (18) | |
| O5 | 0.1946 (5) | 0.1457 (5) | 0.1459 (5) | 0.0208 (16) | |
| O6 | 0.0625 (5) | 0.0865 (5) | 0.1277 (5) | 0.0240 (17) | |
| O7 | 0.0056 (6) | 0.1862 (6) | 0.5922 (6) | 0.033 (2) | |
| O8 | 0.1326 (5) | 0.2550 (5) | 0.5846 (5) | 0.0214 (16) | |
| O9 | 0.3704 (5) | 0.0819 (5) | 0.1997 (5) | 0.0240 (17) | |
| H91 | 0.3822 | 0.0700 | 0.2543 | 0.036* | |
| H92 | 0.4222 | 0.0849 | 0.1778 | 0.036* | |
| O10 | 0.4504 (5) | 0.2736 (5) | 0.2620 (5) | 0.0236 (16) | |
| H101 | 0.4641 | 0.2868 | 0.2082 | 0.035* | |
| H102 | 0.4875 | 0.2327 | 0.2729 | 0.035* | |
| O11 | 0.2668 (7) | 0.0205 (6) | 0.0225 (6) | 0.045 (2) | |
| H111 | 0.2452 | 0.0578 | 0.0593 | 0.068* | |
| H112 | 0.2812 | 0.0241 | −0.0327 | 0.068* | |
| O12 | 0.1257 (7) | −0.0901 (6) | 0.0634 (7) | 0.046 (2) | |
| H121 | 0.0724 | −0.0890 | 0.0818 | 0.068* | |
| H122 | 0.1145 | −0.0821 | 0.0079 | 0.068* | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Tb1 | 0.0145 (3) | 0.0144 (3) | 0.0128 (2) | 0.00004 (17) | −0.00014 (19) | 0.00015 (19) |
| C1 | 0.013 (5) | 0.011 (4) | 0.011 (4) | −0.002 (4) | 0.001 (4) | 0.006 (4) |
| C2 | 0.022 (5) | 0.008 (4) | 0.014 (4) | 0.002 (4) | 0.007 (4) | −0.001 (4) |
| C3 | 0.015 (5) | 0.020 (5) | 0.023 (5) | 0.007 (4) | −0.002 (4) | −0.001 (4) |
| C4 | 0.017 (5) | 0.013 (5) | 0.016 (5) | −0.003 (4) | −0.011 (4) | 0.000 (4) |
| C5 | 0.021 (5) | 0.016 (5) | 0.026 (5) | 0.005 (4) | −0.007 (4) | −0.009 (4) |
| C6 | 0.016 (5) | 0.012 (4) | 0.017 (6) | −0.001 (4) | 0.002 (4) | −0.008 (4) |
| C7 | 0.012 (5) | 0.020 (5) | 0.019 (5) | 0.000 (4) | 0.004 (4) | −0.007 (4) |
| C8 | 0.023 (5) | 0.006 (4) | 0.012 (4) | 0.004 (4) | −0.003 (4) | −0.006 (4) |
| C9 | 0.018 (4) | 0.013 (4) | 0.008 (4) | −0.002 (4) | −0.002 (4) | 0.006 (4) |
| C10 | 0.014 (5) | 0.018 (5) | 0.020 (5) | −0.001 (4) | −0.003 (4) | −0.004 (4) |
| C11 | 0.015 (5) | 0.023 (5) | 0.018 (5) | 0.000 (4) | −0.007 (4) | 0.007 (4) |
| C12 | 0.008 (4) | 0.015 (4) | 0.012 (4) | 0.004 (4) | 0.008 (4) | 0.000 (4) |
| C13 | 0.018 (5) | 0.022 (5) | 0.017 (5) | 0.001 (4) | −0.002 (4) | −0.006 (4) |
| C14 | 0.014 (5) | 0.025 (6) | 0.014 (5) | 0.001 (5) | −0.003 (4) | −0.004 (4) |
| N1 | 0.013 (4) | 0.012 (4) | 0.018 (4) | −0.001 (3) | −0.001 (4) | −0.002 (4) |
| N2 | 0.013 (4) | 0.015 (4) | 0.015 (4) | 0.003 (3) | −0.002 (3) | −0.002 (3) |
| O1 | 0.021 (3) | 0.016 (3) | 0.016 (3) | −0.001 (3) | −0.007 (3) | −0.003 (3) |
| O2 | 0.050 (5) | 0.035 (5) | 0.019 (4) | 0.019 (4) | −0.006 (4) | −0.002 (4) |
| O3 | 0.020 (4) | 0.026 (4) | 0.017 (4) | 0.007 (3) | −0.002 (3) | −0.004 (3) |
| O4 | 0.032 (4) | 0.024 (4) | 0.022 (4) | 0.017 (3) | −0.006 (3) | −0.002 (3) |
| O5 | 0.017 (4) | 0.021 (4) | 0.024 (4) | −0.003 (3) | 0.003 (3) | −0.004 (3) |
| O6 | 0.019 (4) | 0.029 (4) | 0.024 (4) | −0.005 (3) | 0.001 (3) | −0.006 (3) |
| O7 | 0.030 (4) | 0.045 (5) | 0.024 (4) | −0.016 (4) | 0.011 (4) | −0.004 (4) |
| O8 | 0.019 (4) | 0.032 (4) | 0.013 (3) | −0.010 (3) | 0.002 (3) | −0.007 (3) |
| O9 | 0.025 (4) | 0.031 (4) | 0.016 (3) | 0.000 (3) | 0.008 (3) | 0.007 (3) |
| O10 | 0.021 (4) | 0.035 (4) | 0.014 (4) | −0.001 (3) | 0.005 (3) | 0.006 (3) |
| O11 | 0.064 (6) | 0.039 (5) | 0.033 (5) | 0.012 (5) | 0.014 (5) | −0.010 (4) |
| O12 | 0.053 (6) | 0.045 (6) | 0.039 (5) | 0.018 (5) | −0.004 (5) | 0.011 (5) |
Geometric parameters (Å, °) top
| Tb1—O1 | 2.351 (7) | C8—C9 | 1.560 (14) |
| Tb1—O5 | 2.356 (7) | C9—N1 | 1.341 (12) |
| Tb1—O8i | 2.358 (7) | C9—C10 | 1.379 (14) |
| Tb1—O3ii | 2.371 (7) | C10—C11 | 1.368 (16) |
| Tb1—O10 | 2.412 (7) | C10—H10A | 0.930 |
| Tb1—O9 | 2.435 (8) | C11—C12 | 1.435 (14) |
| Tb1—N2 | 2.531 (8) | C11—H11A | 0.930 |
| Tb1—N1 | 2.534 (8) | C12—C13 | 1.359 (14) |
| C1—N2 | 1.335 (13) | C12—C14 | 1.516 (13) |
| C1—C2 | 1.373 (13) | C13—N1 | 1.343 (15) |
| C1—C6 | 1.531 (13) | C13—H13A | 0.930 |
| C2—C3 | 1.393 (15) | C14—O7 | 1.195 (14) |
| C2—H2A | 0.930 | C14—O8 | 1.277 (12) |
| C3—C4 | 1.378 (15) | O1—H1 | 0.850 |
| C3—H3A | 0.930 | O3—Tb1i | 2.371 (7) |
| C4—C5 | 1.370 (15) | O8—Tb1ii | 2.358 (7) |
| C4—C7 | 1.500 (15) | O9—H91 | 0.850 |
| C5—N2 | 1.363 (15) | O9—H92 | 0.850 |
| C5—H5A | 0.930 | O10—H101 | 0.850 |
| C6—O2 | 1.221 (13) | O10—H102 | 0.850 |
| C6—O1 | 1.256 (12) | O11—H111 | 0.850 |
| C7—O4 | 1.226 (13) | O11—H112 | 0.850 |
| C7—O3 | 1.279 (13) | O12—H121 | 0.850 |
| C8—O6 | 1.219 (12) | O12—H122 | 0.850 |
| C8—O5 | 1.242 (13) | | |
| | | |
| O1—Tb1—O5 | 124.7 (3) | O1—C6—C1 | 114.1 (8) |
| O1—Tb1—O8i | 116.1 (3) | O4—C7—O3 | 123.3 (10) |
| O5—Tb1—O8i | 83.7 (2) | O4—C7—C4 | 119.3 (9) |
| O1—Tb1—O3ii | 81.4 (3) | O3—C7—C4 | 117.4 (9) |
| O5—Tb1—O3ii | 116.7 (3) | O6—C8—O5 | 127.2 (10) |
| O8i—Tb1—O3ii | 140.3 (2) | O6—C8—C9 | 117.9 (9) |
| O1—Tb1—O10 | 78.8 (2) | O5—C8—C9 | 114.9 (8) |
| O5—Tb1—O10 | 154.8 (3) | N1—C9—C10 | 121.9 (10) |
| O8i—Tb1—O10 | 76.4 (2) | N1—C9—C8 | 114.6 (9) |
| O3ii—Tb1—O10 | 72.5 (2) | C10—C9—C8 | 123.5 (9) |
| O1—Tb1—O9 | 155.1 (2) | C11—C10—C9 | 119.4 (10) |
| O5—Tb1—O9 | 75.6 (3) | C11—C10—H10A | 120.3 |
| O8i—Tb1—O9 | 77.5 (3) | C9—C10—H10A | 120.3 |
| O3ii—Tb1—O9 | 75.8 (2) | C10—C11—C12 | 120.2 (10) |
| O10—Tb1—O9 | 84.9 (3) | C10—C11—H11A | 119.9 |
| O1—Tb1—N2 | 64.9 (3) | C12—C11—H11A | 119.9 |
| O5—Tb1—N2 | 74.0 (3) | C13—C12—C11 | 114.5 (9) |
| O8i—Tb1—N2 | 73.6 (3) | C13—C12—C14 | 124.7 (10) |
| O3ii—Tb1—N2 | 142.3 (3) | C11—C12—C14 | 120.7 (9) |
| O10—Tb1—N2 | 114.1 (3) | N1—C13—C12 | 126.4 (10) |
| O9—Tb1—N2 | 139.8 (3) | N1—C13—H13A | 116.8 |
| O1—Tb1—N1 | 73.4 (3) | C12—C13—H13A | 116.8 |
| O5—Tb1—N1 | 65.5 (3) | O7—C14—O8 | 124.1 (10) |
| O8i—Tb1—N1 | 145.1 (3) | O7—C14—C12 | 121.0 (10) |
| O3ii—Tb1—N1 | 72.1 (3) | O8—C14—C12 | 114.8 (9) |
| O10—Tb1—N1 | 137.5 (3) | C9—N1—C13 | 117.4 (9) |
| O9—Tb1—N1 | 108.2 (3) | C9—N1—Tb1 | 117.1 (7) |
| N2—Tb1—N1 | 82.1 (3) | C13—N1—Tb1 | 124.5 (7) |
| N2—C1—C2 | 120.3 (9) | C1—N2—C5 | 118.7 (9) |
| N2—C1—C6 | 115.4 (8) | C1—N2—Tb1 | 116.8 (6) |
| C2—C1—C6 | 124.3 (9) | C5—N2—Tb1 | 124.4 (7) |
| C1—C2—C3 | 120.6 (9) | C6—O1—Tb1 | 126.1 (6) |
| C1—C2—H2A | 119.7 | C6—O1—H1 | 116.9 |
| C3—C2—H2A | 119.7 | Tb1—O1—H1 | 117.0 |
| C4—C3—C2 | 119.5 (9) | C7—O3—Tb1i | 141.6 (7) |
| C4—C3—H3A | 120.2 | C8—O5—Tb1 | 127.4 (6) |
| C2—C3—H3A | 120.2 | C14—O8—Tb1ii | 137.7 (6) |
| C5—C4—C3 | 116.8 (9) | Tb1—O9—H91 | 96.6 |
| C5—C4—C7 | 119.9 (9) | Tb1—O9—H92 | 114.0 |
| C3—C4—C7 | 123.3 (9) | H91—O9—H92 | 100.6 |
| N2—C5—C4 | 123.9 (9) | Tb1—O10—H101 | 95.5 |
| N2—C5—H5A | 118.0 | Tb1—O10—H102 | 115.7 |
| C4—C5—H5A | 118.0 | H101—O10—H102 | 100.9 |
| O2—C6—O1 | 126.6 (9) | H111—O11—H112 | 132.5 |
| O2—C6—C1 | 119.3 (9) | H121—O12—H122 | 96.9 |
| | | |
| N2—C1—C2—C3 | −3.4 (15) | O3ii—Tb1—N1—C13 | 41.3 (8) |
| C6—C1—C2—C3 | 174.1 (9) | O10—Tb1—N1—C13 | 6.3 (10) |
| C1—C2—C3—C4 | 0.4 (15) | O9—Tb1—N1—C13 | 109.1 (8) |
| C2—C3—C4—C5 | 3.7 (15) | N2—Tb1—N1—C13 | −111.0 (8) |
| C2—C3—C4—C7 | −175.7 (10) | C2—C1—N2—C5 | 2.2 (14) |
| C3—C4—C5—N2 | −5.2 (16) | C6—C1—N2—C5 | −175.6 (9) |
| C7—C4—C5—N2 | 174.2 (10) | C2—C1—N2—Tb1 | 179.6 (7) |
| N2—C1—C6—O2 | −170.7 (9) | C6—C1—N2—Tb1 | 1.9 (10) |
| C2—C1—C6—O2 | 11.7 (15) | C4—C5—N2—C1 | 2.3 (16) |
| N2—C1—C6—O1 | 10.2 (12) | C4—C5—N2—Tb1 | −174.9 (8) |
| C2—C1—C6—O1 | −167.4 (9) | O1—Tb1—N2—C1 | −7.5 (6) |
| C5—C4—C7—O4 | −178.2 (10) | O5—Tb1—N2—C1 | 134.4 (7) |
| C3—C4—C7—O4 | 1.1 (16) | O8i—Tb1—N2—C1 | −137.6 (7) |
| C5—C4—C7—O3 | −0.4 (15) | O3ii—Tb1—N2—C1 | 21.2 (9) |
| C3—C4—C7—O3 | 178.9 (9) | O10—Tb1—N2—C1 | −71.1 (7) |
| O6—C8—C9—N1 | −171.3 (9) | O9—Tb1—N2—C1 | 176.6 (6) |
| O5—C8—C9—N1 | 7.9 (12) | N1—Tb1—N2—C1 | 67.8 (7) |
| O6—C8—C9—C10 | 10.5 (13) | O1—Tb1—N2—C5 | 169.7 (9) |
| O5—C8—C9—C10 | −170.3 (9) | O5—Tb1—N2—C5 | −48.3 (8) |
| N1—C9—C10—C11 | −3.6 (15) | O8i—Tb1—N2—C5 | 39.7 (8) |
| C8—C9—C10—C11 | 174.4 (9) | O3ii—Tb1—N2—C5 | −161.5 (7) |
| C9—C10—C11—C12 | 3.5 (15) | O10—Tb1—N2—C5 | 106.2 (8) |
| C10—C11—C12—C13 | −0.9 (14) | O9—Tb1—N2—C5 | −6.1 (10) |
| C10—C11—C12—C14 | −177.4 (9) | N1—Tb1—N2—C5 | −115.0 (8) |
| C11—C12—C13—N1 | −1.9 (15) | O2—C6—O1—Tb1 | 161.3 (8) |
| C14—C12—C13—N1 | 174.5 (10) | C1—C6—O1—Tb1 | −19.6 (12) |
| C13—C12—C14—O7 | 178.6 (11) | O5—Tb1—O1—C6 | −30.8 (9) |
| C11—C12—C14—O7 | −5.3 (15) | O8i—Tb1—O1—C6 | 70.2 (8) |
| C13—C12—C14—O8 | −1.4 (14) | O3ii—Tb1—O1—C6 | −147.4 (8) |
| C11—C12—C14—O8 | 174.7 (9) | O10—Tb1—O1—C6 | 138.9 (8) |
| C10—C9—N1—C13 | 1.0 (14) | O9—Tb1—O1—C6 | −171.0 (7) |
| C8—C9—N1—C13 | −177.2 (8) | N2—Tb1—O1—C6 | 15.4 (8) |
| C10—C9—N1—Tb1 | 169.6 (7) | N1—Tb1—O1—C6 | −73.5 (8) |
| C8—C9—N1—Tb1 | −8.6 (10) | O4—C7—O3—Tb1i | 12.3 (17) |
| C12—C13—N1—C9 | 1.8 (16) | C4—C7—O3—Tb1i | −165.4 (7) |
| C12—C13—N1—Tb1 | −165.8 (8) | O6—C8—O5—Tb1 | 176.0 (8) |
| O1—Tb1—N1—C9 | 147.5 (7) | C9—C8—O5—Tb1 | −3.1 (12) |
| O5—Tb1—N1—C9 | 5.4 (6) | O1—Tb1—O5—C8 | −46.5 (9) |
| O8i—Tb1—N1—C9 | 35.5 (9) | O8i—Tb1—O5—C8 | −164.1 (8) |
| O3ii—Tb1—N1—C9 | −126.4 (7) | O3ii—Tb1—O5—C8 | 51.8 (8) |
| O10—Tb1—N1—C9 | −161.3 (6) | O10—Tb1—O5—C8 | 157.8 (7) |
| O9—Tb1—N1—C9 | −58.6 (7) | O9—Tb1—O5—C8 | 117.3 (8) |
| N2—Tb1—N1—C9 | 81.4 (7) | N2—Tb1—O5—C8 | −89.3 (8) |
| O1—Tb1—N1—C13 | −44.8 (8) | N1—Tb1—O5—C8 | −0.9 (8) |
| O5—Tb1—N1—C13 | 173.0 (9) | O7—C14—O8—Tb1ii | 23.9 (17) |
| O8i—Tb1—N1—C13 | −156.8 (7) | C12—C14—O8—Tb1ii | −156.1 (7) |
| Symmetry codes: (i) −x+1/2, −y+1/2, z−1/2; (ii) −x+1/2, −y+1/2, z+1/2. |
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1···O12iii | 0.85 | 1.98 | 2.801 (12) | 162 |
| O9—H91···O4ii | 0.85 | 1.86 | 2.706 (10) | 180 |
| O9—H92···O4iv | 0.85 | 1.99 | 2.842 (11) | 180 |
| O10—H101···O7i | 0.85 | 1.83 | 2.679 (11) | 179 |
| O10—H102···O9iii | 0.85 | 2.15 | 3.000 (11) | 180 |
| O11—H111···O5 | 0.85 | 2.00 | 2.851 (12) | 180 |
| O11—H112···O2i | 0.85 | 1.91 | 2.758 (12) | 180 |
| O12—H121···O6v | 0.85 | 2.15 | 3.000 (12) | 180 |
| O12—H122···O6vi | 0.85 | 2.08 | 2.930 (13) | 180 |
| Symmetry codes: (iii) y+1/2, −x+1/2, −z+1/2; (ii) −x+1/2, −y+1/2, z+1/2; (iv) −y+1, x, −z; (i) −x+1/2, −y+1/2, z−1/2; (v) −x, −y, z; (vi) y, −x, −z. |
Table 1
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1···O12i | 0.85 | 1.98 | 2.801 (12) | 162 |
| O9—H91···O4ii | 0.85 | 1.86 | 2.706 (10) | 180 |
| O9—H92···O4iii | 0.85 | 1.99 | 2.842 (11) | 180 |
| O10—H101···O7iv | 0.85 | 1.83 | 2.679 (11) | 179 |
| O10—H102···O9i | 0.85 | 2.15 | 3.000 (11) | 180 |
| O11—H111···O5 | 0.85 | 2.00 | 2.851 (12) | 180 |
| O11—H112···O2iv | 0.85 | 1.91 | 2.758 (12) | 180 |
| O12—H121···O6v | 0.85 | 2.15 | 3.000 (12) | 180 |
| O12—H122···O6vi | 0.85 | 2.08 | 2.930 (13) | 180 |
| Symmetry codes: (i) y+1/2, −x+1/2, −z+1/2; (ii) −x+1/2, −y+1/2, z+1/2; (iii) −y+1, x, −z; (iv) −x+1/2, −y+1/2, z−1/2; (v) −x, −y, z; (vi) y, −x, −z. |
The authors are grateful for financial support from the Scientific Research
Foundation of Outstanding Talented Persons of Henan Province (grant No.
74200510014).
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The asymmetric unit of the title compound is shown in Fig. 1. Atom Tb1 displays octa-coordination through two water molecules, four carboxylate O atoms and two pyridyl N atoms from two 2,5-pydc and two 2,5-Hpydc ligands (2,5-pydc = pyridine-2,5-dicarboxylate). The 2,5-pydc and 2,5-Hpydc ligands bridge between TbIII atoms to generate helical coordination polymers along [001] (Fig. 2). An extensive network of O—H···O hydrogen bonds is formed between the coordination polymers and the lattice water molecules (Table 1 and Fig. 3).